A new macrocyclic ligand, 1,3,5-triaza-2,4:7,8:13,14-tribenzo-9,12-dioksa-cyclopentadeca-1,5-diene was synthesized by reaction of 2,6-diaminopyridine and 1,2-bis(2-carboxyaldehyde phenoxy)ethane. Then, its Cu(II), Ni(II), Pb(II), Co(III) and La(III) complexes were synthesized by the template effect by the reaction of 2,6-diaminopyridine and 1,2-bis(2-carboxyaldehyde phenoxy)ethane and Cu(NO3)2 · 3H2O, Ni(NO3)2 · 6H2O, Pb(NO3)2, Co(NO3)2 · 6H2O, La(NO3)3 · 6H2O, respectively. The ligand and its metal complexes have been characterized by elemental analysis, IR, 1H and 13C NMR, UV-Vis spectra, magnetic susceptibility, thermal gravimetric analysis, conductivity measurements, mass spectra, and cyclic voltammetry. All complexes are diamagnetic and Cu(II) complex is binuclear. The Co(II) was oxidized to Co(III). The comparative electrochemical studies show that the nickel complex exhibited a quasi-reversible one-electron reduction process, while copper and cobalt complexes gave irreversible reduction processes in DMSO solution. 相似文献
Recently the connection between oxidative stress and various diseases, including cancer and Alzheimer's, attracts notice as a pathway suitable for diagnostic purposes. 8‐Oxo‐deoxyguanosine and 8‐oxo‐deoxyadenosine produced from the interaction of reactive oxygen species with DNA become prominent as biomarkers. Several methods have been developed for their determination in biofluids, including solid‐phase extraction and enzyme‐linked immunosorbent assays. However, still, there is a need for reliable and fast analytical methods. In this context, solid‐phase microextraction offers many advantages such as flexibility in geometry and applicable sample volume, as well as high adaptability to high‐throughput sampling. In this study, a solid‐phase microextraction method was developed for the determination of 8‐oxo‐deoxyguanosine and 8‐oxo‐deoxyadenosine in biofluids. The extractive phase of solid‐phase microextraction consisted of hydrophilic–lipophilic balanced polymeric particles. In order to develop a solid‐phase microextraction method suitable for the determination of the analytes in saliva and urine, several parameters, including desorption solvent, desorption time, sample pH, and ionic strength, were scrutinized. Analytical figures of merit indicated that the developed method provides reasonable interday and intraday precisions (<15% in both biofluids) with acceptable accuracy. The method provides a limit of quantification for both biomarkers at 5.0 and 10.0 ng/mL levels in saliva and urine matrices, respectively. 相似文献
This research was focused on the preparation of mixed metal oxide pigments doped with terbium ions with the general formula of Sn0.752Co0.08P0.16Tb0.008O2. These pigments were synthesised by solid-state reactions at high calcination temperatures. The temperature range was chosen from 1350 to 1500 °C. The goal was to develop conditions for the synthesis of this type of pigments and to determine the influence of terbium ions on the colour properties of these compounds. All prepared pigments were applied into the organic matrix and into the ceramic glaze. Thermal behaviours of the reaction mixtures were investigated using differential thermal and thermogravimetric analysis. Synthesised Sn0.752Co0.08P0.16Tb0.008O2 pigments were compared with concurrently prepared pigment Sn0.760Co0.08P0.16O2 depending on the calcination temperature with respect to the colour properties in CIE L*a*b* colour space, furthermore from the point of particle size distribution and phase composition. All compounds provided blue–violet hues that are stable in ceramic glazes. 相似文献
Sailing the seven ‘C's : 2,2,3‐Trimethylbutane (triptane) selectively forms from dimethyl ether at low temperatures on acid zeolites. Selective methylation at less‐substituted carbons, relative rates of methylation to hydrogen transfer as a function of chain size, slow skeletal isomerization, and β‐scission cracking of triptyl chains and their precursors are intrinsic properties of carbenium ions and account for the remarkable triptane selectivities within C7 .
In this study, synthesis of poly(epichlorohydrin-g-methyl methacrylate) graft copolymers by reversible addition-fragmentation chain transfer (RAFT) polymerization was reported. For this purpose, epichlorohydrin was polymerized by using HNO3 via cationic ring-opening mechanism. A RAFT macroinitiator (macro-RAFT agent) was obtained by the reaction of potassium ethyl xanthogenate and polyepichlorohydrin. The graft copolymers were synthesized using macro-RAFT agent as initiator and methyl methacrylate as monomer. The synthesis of graft copolymers was conducted by changing the time of polymerization and the amount of monomer-initiator concentration that affect the RAFT polymerization. The effects of these parameters on polymerization were evaluated via various analyses. The characterization of the products was determined using 1H-nuclear magnetic resonance (1H-NMR), Fourier-transform infrared spectroscopy, gel-permeation chromatography, thermogravimetric analysis, elemental analysis, and fractional precipitation techniques. The block lengths of the graft copolymers were calculated by using 1H-NMR spectrum. It was observed that the block length could be altered by varying the monomer and initiator concentrations. 相似文献